Anda di halaman 1dari 5

American Association State

Highway and Transportation Officials Standard


AASHTO No.: T78

Designation: D 402 02

27/74 (88)

Standard Test Method for

Distillation of Cut-Back Asphaltic (Bituminous) Products1


This standard is issued under the fixed designation D 402; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense. This method was adopted as a joint ASTM-IP
standard in 1961.

3. Summary of Method
3.1 Two hundred millilitres of the sample are distilled in a
500-mL flask, at a controlled rate, to a temperature in the liquid
of 360C (680F), and the volumes of distillate obtained at
specified temperatures are measured. The residue from the
distillation, and also the distillate, may be tested as required.

1. Scope
1.1 This test method covers a distillation test for cut-back
asphaltic (bituminous) products.
1.2 The values given in SI units are to be regarded as the
standard. The inch-pound units given in parentheses are for
information only.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

4. Significance and Use


4.1 This procedure measures the amount of the more volatile constituents in cut-back asphaltic products. The properties
of the residue after distillation are not necessarily characteristic
of the bitumen used in the original mixture, nor of the residue
which may be left at any particular time after field application
of the cut-back asphaltic product. The presence of silicone in
the cut-back may affect the distillation residue by retarding the
loss of volatile material after the residue has been poured into
the residue container.

2. Referenced Documents
2.1 ASTM Standards:
D 86 Test Method for Distillation of Petroleum Products at
Atmospheric Pressure2
D 370 Test Method for Dehydration of Oil-Type Preservatives3
E 1 Specification for ASTM Thermometers4
E 133 Specification for Distillation Equipment5
E 220 Test Method for Calibration of Thermocouples by
Comparison Techniques4
2.2 IP Standards:
IP 123/ASTM D 86, Distillation of Petroleum Products
Thermometers as specified in IP Standards
Crow Receiver as specified in British Standards 658:1989
C.O.3Standard Methods for Testing Tar and its Products
(Published by the U.K. Standardization of Tar Products
Tests Committee)

5. Apparatus
5.1 Distillation Flask, 500-mL side-arm, having the dimensions shown in Fig. 1.
5.2 Condenser, standard glass-jacketed, of nominal jacket
length from 200 to 300 mm and overall tube length of 450 6
10 mm (see Fig. 3).
5.3 Adapter, heavy-wall (1-mm) glass, with reinforced top,
having an angle of approximately 105. The inside diameter at
the large end shall be approximately 18 mm, and at the small
end, not less than 5 mm. The lower surface of the adapter shall
be on a smooth descending curve from the larger end to the
smaller. The inside line of the outlet end shall be vertical, and
the outlet shall be cut or ground (not fire-polished) at an angle
of 45 6 5 to the inside line.
5.4 Shield, steel, lined with 3-mm fire proof insulation and
fitted with transparent mica windows, of the form and dimensions shown in Fig. 2, used to protect the flask from air currents
and to reduce radiation. The cover (top) shall be made in two
parts of 6.4-mm fire proof insulation.
5.5 Shield and Flask SupportTwo 15-cm2 sheets of 16mesh Chromel wire gauze on a tripod or ring.

1
This test method is under the jurisdiction of ASTM Committee D04 on Road
and Paving Materials and is the direct responsibility of Subcommittee D04.46 on
Durability and Distillation Tests.
Current edition approved Dec. 10, 2002. Published February 2003. Originally
approved in 1934. Last previous edition approved in 1997 as D 402 97.
In the IP, this method is under the jurisdiction of the Standardization Committee.
2
Annual Book of ASTM Standards, Vol 05.01.
3
Annual Book of ASTM Standards, Vol 04.09.
4
Annual Book of ASTM Standards, Vol 14.03.
5
Annual Book of ASTM Standards, Vol 14.02.

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

D 402 02

FIG. 1 Distillation Flask

FIG. 2 Shield

5.6 Heat Source


5.6.1 Adjustable Tirrill-type gas burner or equivalent.
5.6.2 An electric heater equipped with a transformer capable of controlling from 0 to 750 W. The shield and support
shall be a refractory with an opening of 79 mm, with the upper
surface beveled to 86 mm to accommodate the specified
500-mL flask. When the flask is placed on the refractory, there
should be a distance of approximately 3 mm between the
bottom of the flask and the heating elements.

5.7 ReceiverA standard 100-mL graduated cylinder conforming to dimensions of Specification E 133, or a 100-mL
Crow receiver as shown in Fig. 4 of this test method.
NOTE 1Receivers of smaller capacity having 0.1-mL divisions may
be used when low volumes of total distillate are expected and the added
accuracy required.

D 402 02

FIG. 3 Distillation Apparatus

pour this back into the flask when the contents have cooled just
sufficiently to prevent loss of volatile oil. Mix the contents of
the flask thoroughly before removal for analysis. An alternative
procedure is described in Test Method D 370.
7. Preparation of Apparatus
7.1 Calculate the weight of 200 mL of the sample from the
specific gravity of the material at 15.6/15.6C. Weigh this
amount 6 0.5 g into the 500-mL flask.
7.2 Place the flask in the shield supported by two sheets of
gauze on a tripod or ring. Connect the condenser tube to the
tubulature of the flask with a tight cork joint. Clamp the
condenser so that the axis of the bulb of the flask through the
center of its neck is vertical. Adjust the adapter over the end of
the condenser tube so that the distance from the neck of the
flask to the outlet of the adapter is 650 6 50 mm (see Fig. 3).
7.3 Insert the thermometer through a tightly fitting cork in
the neck of the flask so that the bulb of the thermometer rests
on the bottom of the flask. Raise the thermometer 6 mm from
the bottom of the flask using the scale divisions on the
thermometer to estimate the 6 mm distance above the top of the
cork.
7.4 Protect the burner by a suitable shield or chimney. Place
the receiver so that the adapter extends at least 25 mm but not
below the 100-mL mark. Cover the graduate closely with a
piece of blotting paper, or similar material, suitably weighted,
which has been cut to fit the adapter snugly.
7.5 The flask, condenser tube, adapter, and receiver shall be
clean and dry before starting the distillation. Place the seamless
residue container on its cover in an area free from drafts.
7.6 Pass cold water through the condenser jacket. Use warm
water if necessary to prevent formation of solid condensate in
the condenser tube.

All dimensions are in millimetres

FIG. 4 Crow Receivers of Capacity 25, 50, and 100 mL

5.8 Residue ContainerA seamless metal container with


slip on cover of 75 6 5 mm in diameter, and 55 6 5 mm in
height.
5.9 Thermometer ASTM High Distillation Thermometers
having a range from 6 to 400C (20 to 760F) and conforming
to the requirements for Thermometers 8C (8F) as prescribed in
Specification E 1, or IP Thermometer 6C conforming to IP
Specifications for Standard Thermometers, or an equivalent
thermometric device that has been calibrated in accordance
with Test Method E 220. ASTM 8C Thermometers shall be
used for referee testing.
6. Sampling
6.1 Stir the sample thoroughly, warming if necessary, to
ensure homogeneity before removal of a portion for analysis.
6.2 If sufficient water is present to cause foaming or
bumping, dehydrate a sample of not less than 250 mL by
heating in a distillation flask sufficiently large to prevent
foaming over into the side arm. When foaming has ceased, stop
the distillation. If any light oil has distilled over, separate and

8. Procedure
8.1 Correct the temperatures to be observed in the distillation if the elevation of the laboratory at which the distillation
is made deviates 150 m or more from sea level. Corrected
3

D 402 02
TABLE 2 Corrected Distillation Temperatures for Various
Altitudes, F

temperatures for the effect of altitude are shown in Table 1 and


Table 2. If the prevailing barometric pressure in millimetres of
mercury is known, correct the temperature to be observed with
the corrections shown in Table 3. Do not correct for the
emergent stem of the thermometer.

Elevation above
sea level, m (ft)
300
150
0
150
300
450
600
750
900
1050
1200
1350
1500
1650
1800
1950
2100
2250
2400

NOTE 2Table 3 covers a wide range of temperatures from 160 to


360C (320 to 680F) and is to be preferred for world-wide specifications
other than ASTM/IP specifications.

8.2 Apply heat so that the first drop of distillate falls from
the end of the flask side-arm in 5 to 15 min. Conduct the
distillation so as to maintain the following drop rates, the drop
count to be made at the tip of the adapter:
50 to 70 drops per minute to 260C (500F)
20 to 70 drops per minute between 260 and 316C (500 and 600F)
Not over 10 min to complete distillation from 316 to 360C (600 to 680F)

8.2.1 Record the volumes of distillate to the nearest 0.5 mL


in the receiver at the corrected temperatures. If the volume of
distillate recovered is critical, use receivers graduated in
0.1-mL divisions and immersed in a transparent bath maintained at 15.6 6 3C.

8.3 When the temperature reaches the corrected temperature


of 360C (680F), cut off the heat and remove the flask and
thermometer. With the flask in a pouring position, remove the
thermometer and immediately pour the contents into the
residue container. The total time from cutting off the heat to
starting the pour shall not exceed 30 s. When pouring, the
side-arm should be substantially horizontal to prevent condensate in the side-arm from being returned to the residue.

Distillation Temperatures for Various Altitudes, C


227
226
225
224
223
223
222
221
220
220
219
218
218
217
216
216
215
214
214

262
261
260
259
258
257
257
256
255
254
254
253
252
251
250
250
249
248
248

318
317
316
315
314
313
312
311
311
310
309
308
307
306
306
305
304
303
303

503
502
500
499
497
495
494
493
491
490
488
487
486
484
483
482
481
479
478

604
602
600
598
597
595
593
592
590
589
587
586
584
583
581
580
579
577
576

684
682
680
678
676
675
673
671
669
668
666
665
663
661
660
658
657
655
654

Nominal Temperatures,
C (F)

CorrectionA per 10 mm Hg
Difference in Pressure,
C (F)

160 (320)
175 (347)
190 (374)
225 (437)
250 (482)
260 (500)
275 (527)
300 (572)
315.6 (600)
325 (617)
360 (680)

0.514 (0.925)
0.531 (0.957)
0.549 (0.989)
0.591 (1.063)
0.620 (1.116)
0.632 (1.138)
0.650 (1.170)
0.680 (1.223)
0.698 (1.257)
0.709 (1.277)
0.751 (1.351)

8.4 Allow the condenser and any distillates trapped in the


condenser neck to drain into the receiver and record the total
volume of distillate collected as total distillate to 360C
(680F).
8.5 When the residue has cooled until fuming just ceases,
stir thoroughly and then, when the material reaches 135 6 5C
(275 6 9F), pour into the receptacles for testing for properties
such as penetration, viscosity, or softening point. Proceed as
required by the appropriate ASTM or IP method from the point
that follows the pouring stage.
8.6 If desired, the distillate, or the combined distillates from
several tests, may be submitted to a further distillation, in
accordance with Test Method D 86 IP 123, or, when the
distillate is of coal-tar origin, Method C.O.3.

TABLE 1 Corrected Distillation Temperatures for Various


Altitudes, C

192
191
190
189
189
188
187
186
186
185
184
184
183
182
182
181
180
180
179

440
438
437
436
434
433
431
430
429
427
426
425
424
422
421
420
419
418
416

A
To be subtracted in case the barometric pressure is below 760 mm Hg; to be
added in case barometric pressure is above 760 mm Hg.

NOTE 4The formation of skin on the surface of a residue during


cooling entraps vapors which will condense and cause higher penetration
results when they are stirred back into the sample. If skin begins to form
during cooling, it should be gently pushed aside. This can be done with a
spatula with a minimum of disturbance to the sample.

300
150
0
150
300
450
600
750
900
1050
1200
1350
1500
1650
1800
1950
2100
2250
2400

377
375
374
373
371
370
369
368
366
365
364
363
362
360
359
358
357
356
355

TABLE 3 Factors for Calculating Temperature Corrections

NOTE 3Some cut-back asphaltic products yield either no distillate or


very little distillate over portions of the temperature range to 316C
(600F). In this case it becomes impractical to maintain the above
distillation rates. For such cases the intent of the method shall be met if the
rate of rise of temperature exceeds 5C (9F)/min.

Elevation above
Sea Level, m

Distillation Temperatures for Various Altitudes, F

362
361
360
359
358
357
356
355
354
353
352
351
351
350
349
348
347
346
346

9. Calculation and Report


9.1 Asphaltic ResidueCalculate the percent residue to the
nearest 0.1 as follows:
R 5 @~200 2 TD!/200# 3 100

where:
R = residue content, in volume percent, and
TD = total distillate recovered to 360C (680F), mL.
4

(1)

D 402 02
9.4 Where penetration, viscosity, or other tests have been
carried out, report with reference to this test method as well as
to any other method used. ExamplePenetration (ASTM D5
or IP 49) of residue from ASTM D402/IP 27.

9.1.1 Report as the residue from distillation to 360 (680F),


percent volume by difference.
9.2 Total Distillate Calculate the percent total distillate to
the nearest 0.1 as follows:
TD % 5 ~TD/200! 3 100

(2)

10. Precision and Bias

9.2.1 Report as the total distillate to 360C (680F), volume


percent.
9.3 Distillate Fractions:
9.3.1 Determine the percentages by volume of the original
sample by dividing the observed volume (in millilitres) of the
fraction by 2. Report to the nearest 0.1 as volume percent as
follows:
Up to 190C (374F)
Up to 225C (437F)
Up to 260C (500F)
Up to 316C (600F)
9.3.2 Determine the percentages by volume of total distillate by dividing the observed volume in millilitres of the
fraction by the millilitres recovered to 360C (680F) and
multiplying by 100. Report to the nearest 0.1 as the distillate,
volume percent of total distillate to 360C (680F) as follows:
Up
Up
Up
Up

to
to
to
to

190C
225C
260C
316C

10.1 The following criteria shall be used for judging the


acceptability of results (95 % probability):
10.1.1 Repeatability Duplicate values by the same operator shall not be considered suspect unless the determined
percentages differ by more than 1.0 volume % of the original
sample.
10.1.2 Reproducibility The values reported by each of
two laboratories, shall not be considered suspect unless the
reported percentages differ by more than the following:
Distillation Fractions, volume percent of the original sample:
Up to 175C (347F)
Above 175C (347F)
Residue, Volume percentage by difference from the original sample

3.5
2.0
2.0

10.2 Criteria for judging variability of test results on the


distillation residue have not been determined.

(374F)
(437F)
(500F)
(600F)

11. Keywords
11.1 cut-back asphalt; distillate; residue

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).